US11105774B2 - Light-assisted quartz crystal microbalance and measurement method thereof - Google Patents
Light-assisted quartz crystal microbalance and measurement method thereof Download PDFInfo
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- US11105774B2 US11105774B2 US16/763,231 US201716763231A US11105774B2 US 11105774 B2 US11105774 B2 US 11105774B2 US 201716763231 A US201716763231 A US 201716763231A US 11105774 B2 US11105774 B2 US 11105774B2
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- 238000003380 quartz crystal microbalance Methods 0.000 title claims abstract description 146
- 238000000691 measurement method Methods 0.000 title abstract 2
- 238000000961 QCM-D Methods 0.000 claims abstract description 89
- 239000013078 crystal Substances 0.000 claims abstract description 37
- 239000010453 quartz Substances 0.000 claims abstract description 37
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 37
- 230000010355 oscillation Effects 0.000 claims abstract description 9
- 238000001514 detection method Methods 0.000 claims description 52
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- 230000005684 electric field Effects 0.000 claims description 6
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- 238000000034 method Methods 0.000 claims description 6
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- 239000004033 plastic Substances 0.000 claims description 3
- 230000035945 sensitivity Effects 0.000 abstract description 16
- 238000005259 measurement Methods 0.000 abstract 1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 12
- 239000000243 solution Substances 0.000 description 4
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- 238000011898 label-free detection Methods 0.000 description 2
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- 150000003384 small molecules Chemical class 0.000 description 1
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Images
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N29/00—Investigating or analysing materials by the use of ultrasonic, sonic or infrasonic waves; Visualisation of the interior of objects by transmitting ultrasonic or sonic waves through the object
- G01N29/02—Analysing fluids
- G01N29/022—Fluid sensors based on microsensors, e.g. quartz crystal-microbalance [QCM], surface acoustic wave [SAW] devices, tuning forks, cantilevers, flexural plate wave [FPW] devices
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N29/00—Investigating or analysing materials by the use of ultrasonic, sonic or infrasonic waves; Visualisation of the interior of objects by transmitting ultrasonic or sonic waves through the object
- G01N29/02—Analysing fluids
- G01N29/036—Analysing fluids by measuring frequency or resonance of acoustic waves
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N29/00—Investigating or analysing materials by the use of ultrasonic, sonic or infrasonic waves; Visualisation of the interior of objects by transmitting ultrasonic or sonic waves through the object
- G01N29/22—Details, e.g. general constructional or apparatus details
- G01N29/222—Constructional or flow details for analysing fluids
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N29/00—Investigating or analysing materials by the use of ultrasonic, sonic or infrasonic waves; Visualisation of the interior of objects by transmitting ultrasonic or sonic waves through the object
- G01N29/22—Details, e.g. general constructional or apparatus details
- G01N29/32—Arrangements for suppressing undesired influences, e.g. temperature or pressure variations, compensating for signal noise
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2291/00—Indexing codes associated with group G01N29/00
- G01N2291/01—Indexing codes associated with the measuring variable
- G01N2291/014—Resonance or resonant frequency
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2291/00—Indexing codes associated with group G01N29/00
- G01N2291/02—Indexing codes associated with the analysed material
- G01N2291/025—Change of phase or condition
- G01N2291/0255—(Bio)chemical reactions, e.g. on biosensors
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2291/00—Indexing codes associated with group G01N29/00
- G01N2291/02—Indexing codes associated with the analysed material
- G01N2291/025—Change of phase or condition
- G01N2291/0256—Adsorption, desorption, surface mass change, e.g. on biosensors
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2291/00—Indexing codes associated with group G01N29/00
- G01N2291/04—Wave modes and trajectories
- G01N2291/042—Wave modes
- G01N2291/0426—Bulk waves, e.g. quartz crystal microbalance, torsional waves
Definitions
- the invention relates to the technical field of instruments and meters, in particular to a novel light-assisted quartz crystal microbalance and a detection method thereof.
- ⁇ ⁇ ⁇ f - 2 ⁇ f 0 2 ⁇ ⁇ ⁇ ⁇ m A ⁇ ⁇ q ⁇ ⁇ q
- ⁇ f is the frequency variation (Hz)
- ⁇ m is the variation of the surface quality of the chip (g)
- f 0 is the resonant frequency of the QCM chip (Hz)
- A is the area of the reactive-electrode of the QCM chip (cm 2 )
- ⁇ q is the density (2.65 g/cm 3 )
- ⁇ q is the shear modulus.
- Quartz crystal microbalances are widely used in various fields, such as monitoring surface thickness in vacuum. This application also greatly expands the application of quartz crystal microbalances as sensors in other fields, such as detection of atmospheric pollutants, metal corrosion and protection, phase transition of polymers, and biosensing detection, etc.
- Quartz crystal microbalances are a powerful label-free detection technique, and have received more and more attention in various fields.
- quartz crystal microbalances are under development compared with another label-free detection technique—surface plasma resonance (SPR).
- SPR surface plasma resonance
- One of the important reasons for the great commercial success of the SPR technique is that the detection sensitivity of a SPR system is generally higher than that of a quartz crystal microbalance.
- the sensitivity of a 5 MHz quartz crystal microbalance is about 20 times lower than that of the corresponding SPR system.
- the signals of a quartz crystal microbalance are not strong enough to obtain relevant information of the detection object.
- the sensitivity of a quartz crystal microbalance is defined as the mass change on unit surface area of a QCM chip corresponding to certain signal change.
- the detection sensitivity is related with the density of the surface detection object, the inherent resonant frequency of the chip, and the shear modulus. According to the Sauerbrey equation, for a 5 MHz AT-cut quartz crystal microbalance chip, the detection sensitivity is about 17.7 ng/cm 2 for 1 Hz of frequency variation.
- Increasing the resonant frequency of a quartz crystal microbalance chip can promote the improvement of the detection sensitivity of the quartz crystal microbalance, but will lead to higher requirements for the manufacturing of ultra-thin quartz crystal chips, because ultra-thin quartz crystal chips are very fragile. Therefore, there are some limitations on improving the detection sensitivity by reducing the thickness of the quartz crystal chip. Owing to these limitations, at present, most manufacturers of quartz crystal microbalances improve the resolution of the detection signals by optimizing the circuits, and finally reduce the limit of detection (LOD), which is the minimum detectable changing value of the concentration or mass of the detection object, and is related with the detection sensitivity and the accuracy of the signals.
- LOD limit of detection
- the LOD of a quartz crystal microbalance is lower than 1 ng/cm 2 , and such a LOD can't fully meet the application requirements.
- the concentration of the detection objects is at ng/mL level. Therefore, it is an urgent task to improve the sensitivity and LOD of quartz crystal microbalances.
- the present invention intends to provide a quartz crystal microbalance system which has higher detection sensitivity without reducing the thickness of the chip and causing chip breakage, and a detection method thereof; besides, the present invention can also improve the detection sensitivity of the quartz crystal microbalance system.
- a novel light-assisted quartz crystal microbalance comprising the following parts:
- a QCM/QCM-D chip which has a sandwich structure formed by a quartz crystal wafer sandwiched between two pieces of electrodes, wherein the chip and the electrode circuit are encapsulated by a metal, ceramic or plastic shell and form a reaction chamber, and the chip and the shell integrally form a quartz crystal resonator;
- an oscillation circuit for providing an alternating electric field for the quartz crystal in the QCM/QCM-D chip
- a frequency counter for monitoring the resonant frequency of the QCM/QCM-D chip
- a light source capable of irradiating light on the surface of the QCM/QCM-D chip.
- the light source is a light source having one or more frequencies.
- a grating unit is arranged between the light source and the QCM/QCM-D chip, and is configured to control the irradiation of the light from the light source on the surface of the QCM/QCM-D chip.
- the grating unit comprises a movable grating baffle and a driver capable of moving the grating baffle.
- the grating baffle is a removable grating baffle, and the driver is an electric driver.
- the novel light-assisted quartz crystal microbalance also contains a computer, which is connected with the driver of the grating baffle, the oscillation circuit and the frequency counter, and is configured to control the operation of the driver of the grating baffle to move the grating baffle, to control the on-off of the oscillation circuit and parameters of electric field, to read the data collected by the frequency counter, and to obtain the change of the resonant frequency of the QCM/QCM-D chip in the detection process.
- a computer which is connected with the driver of the grating baffle, the oscillation circuit and the frequency counter, and is configured to control the operation of the driver of the grating baffle to move the grating baffle, to control the on-off of the oscillation circuit and parameters of electric field, to read the data collected by the frequency counter, and to obtain the change of the resonant frequency of the QCM/QCM-D chip in the detection process.
- the wavelength range of the light generated by the light source is 100-800 nm, preferably is 200-400 nm.
- a detection method of the novel light-assisted quartz crystal microbalance comprising the following steps:
- step 1 operating the quartz crystal microbalance system, and acquiring a stable baseline of the resonant frequency of the QCM/QCM-D chip via the frequency counter;
- step 2 turning on the switch of the light source to irradiate light to the surface of the QCM/QCM-D chip, and obtaining the resonant frequency of the QCM/QCM-D chip as signal 1 via the frequency counter;
- step 3 stopping the irradiation of the light from the light source on the surface of the QCM/QCM-D chip;
- step 4 pushing the object to be detected to the surface of the QCM/QCM-D chip, then making the light irradiate on the surface of the QCM/QCM-D chip, obtaining the resonant frequency of the QCM/QCM-D chip as signal 2 via the frequency counter, and comparing the difference between the signal 1 and the signal 2 .
- the grating unit is arranged between the light source and the QCM/QCM-D chip, so as to control irradiation of the light from the light source on the surface of the QCM/QCM-D chip.
- the detection method of the quartz crystal microbalance is applicable to gas and liquid detection objects, and the quartz crystal resonator is used for accommodating the gas or liquid in the environment in which the detection object is located and the detection object.
- a light source capable of irradiating light to the surface of the chip is additionally arranged, the surface properties of the QCM/QCM-D chip are changed under the light irradiation, and a water molecule layer absorbed on the surface of the QCM/QCM-D chip is reversibly desorbed from the electrode surface of the QCM/QCM-D chip; the irradiation of the light from the light source on the surface of the QCM/QCM-D chip can cause sharp rise of the resonant frequency. Accordingly, the light irradiation on the surface of the chip also causes changes of the mechanical properties and piezoelectric properties of the quartz crystal, and thereby the detection sensitivity of the quartz crystal microbalance system is effectively improved.
- a grating unit is used to control the irradiation of the light from the light source on the surface of the chip. Compared with a light irradiation control scheme that simply relies on switching on/off the light source, the grating unit can quickly, effectively and accurately control the light irradiation on the surface of the QCM/QCM-D chip.
- the detection objects may include compounds of different concentrations and different kinds and cover various chemicals and biomolecules, such as tumor diagnostic markers.
- FIG. 1 is a schematic diagram of the QCM sensor system according to the present invention.
- FIG. 2A is a schematic diagram of the general process of detecting PBS solutions at different concentrations flowing across the surface of the chip with a curve of QCM resonant frequency which changes over time under the switching control of the grating unit;
- FIG. 2B is a data graph for detecting PBS solutions at different concentrations flowing across the surface of the chip as the QCM resonant frequency changes over time, with the light irradiating on the surface of the QCM/QCM-D chip under switch control of the grating unit;
- FIG. 3 is a data graph for detecting PBS solutions at different concentrations flowing across the surface of the chip as the curve of the QCM/QCM-D resonant frequency changes over time, without light irradiation on the surface of the QCM/QCM-D chip.
- the novel light-assisted quartz crystal microbalance 2 comprises a quartz crystal microbalance/quartz crystal microbalance with dissipation (QCM/QCM-D) chip, which has a sandwich structure that is formed by a quartz crystal wafer layer 16 sandwiched between two pieces of electrodes, wherein the chip and the electrode circuit are encapsulated by a metal, ceramic or plastic shell and form a reaction chamber 14 , the chip and the shell integrally form a quartz crystal resonator, and the QCM/QCM-D chip 20 is installed in a groove 18 at the bottom surface of the reaction chamber 14 , the reaction chamber 14 is used for accommodating the gas or liquid in the environment in which the detection object is located and the detection object; an oscillation circuit for providing an alternating electric field for the quartz crystal wafer layer 16 in the QCM/QCM-D chip 20 ; a frequency counter 22 for monitoring the resonant frequency of the QCM/QCM-D chip 20 ; and a light source 6 capable
- the light source 6 is a light source having one or more frequencies, and can generate light within a wavelength range of 100-800 nm, preferably 200-400 nm, such as 365 nm. A better effect can be attained if the frequency of the light emitted from the light source 6 is lower or the energy and power of the irradiated emitted light are higher.
- the surface properties of the QCM/QCM-D chip 20 are changed, and the water molecules absorbed on the surface of the QCM/QCM-D chip are reversibly desorbed from the surface of the QCM/QCM-D chip 20 , thus the resonant frequency of the QCM/QCM-D chip is increased. Accordingly, the light irradiation on the surface of the chip also causes changes of the mechanical properties and piezoelectric properties of the quartz crystal in the chip, and thereby the detection sensitivity of the equipment system of the quartz crystal microbalance 2 is effectively improved. By applying the light source 6 , the sensitivity of the system of the quartz crystal microbalance 2 can be improved by ten times or more.
- the novel light-assisted quartz crystal microbalance 2 comprises a grating unit 10 disposed between the light source 6 and the QCM/QCM-D chip 20 for controlling the irradiation of the light 12 from the light source 6 on the surface of the QCM/QCM-D chip 20 .
- the grating unit 10 comprises a movable grating baffle 8 and a driver for changing the position of the baffle 8 .
- a variety of drivers are available, and an electric driver can be selected.
- the grating baffle 8 is removable.
- the grating baffle 8 can provide more protection and block the irradiation of the light emitted from the light source 6 on the surface of the QCM/QCM-D chip 20 .
- the driver is advantageously controlled by a control unit installed in the computer 4 .
- the opening or closing of the grating unit 10 can be controlled by the computer 4 connected to the grating unit 10 through the software installed on the computer 4 , so as to control the light 12 irradiating the surface of the QCM/QCM-D chip 20 .
- the computer 4 is connected to the reaction chamber 14 of the quartz crystal resonator and the frequency counter 22 to control the oscillation circuit and electric field parameters, read the data collected by the frequency counter 22 , and to obtain the change of the resonant frequency of the QCM/QCM-D chip in the detection process.
- the detection method of the novel light-assisted quartz crystal microbalance 2 according to the present invention comprises the following steps:
- step 1 operating the system of the quartz crystal microbalance 2 , and acquiring a stable baseline of the resonant frequency of the quartz crystal in the QCM/QCM-D chip 20 via the frequency counter 22 ;
- step 2 turning on the switch of the light source 6 to irradiate light to the surface of the QCM/QCM-D chip 20 , and obtaining the resonant frequency of the quartz crystal of the QCM/QCM-D chip 20 as signal 1 via the frequency counter 22 ;
- step 3 stopping the irradiation of the light from the light source 6 on the surface of the QCM/QCM-D chip 20 ;
- step 4 pushing the object to be detected to the surface of the QCM/QCM-D chip 20 , then making the light 12 irradiate on the surface of the QCM/QCM-D chip 20 , obtaining the resonant frequency of the QCM/QCM-D chip 20 as signal 2 via the frequency counter 22 , and comparing the difference between the signal 1 and the signal 2 .
- the grating unit 10 is arranged between the light source 6 and the QCM/QCM-D chip 2 to control irradiation of the light 12 of the light source 6 on the surface of the QCM/QCM-D chip 20 .
- the irradiation of the light on the surface of the QCM/QCM-D chip 20 can be controlled quickly, effectively and accurately, and the grating unit 10 is much faster and more efficient than a simple control scheme that simply relies on the on-off control of the light source 6 .
- the detection method can be performed in gas or liquid state, and the chamber 12 is used for accommodating the gas or liquid in the environment in which the detection object is located and the detection object.
- the detected objects can include compounds of different concentrations and different kinds and cover various chemicals and biomolecules, such as tumor diagnostic markers.
- FIG. 2A is a schematic diagram showing the general process of detecting a liquid sample with the novel light-assisted quartz crystal microbalance 2 according to the present invention on the basis of the change of the resonant frequency of the quartz crystal over time, when the grating unit 10 is turned on and off.
- Time a represents the operation of “injecting water” to the surface of the QCM/QCM-D chip 20 . Before water is injected, the resonant frequency of the quartz crystal is the highest, and only air exists on the surface of the QCM/QCM-D chip 20 in this period. After water is injected to the surface of the QCM/QCM-D chip 20 , the frequency will drop to a lower value.
- Time b represents the operation of “opening the grating”.
- Time c represents the operation of “closing the grating”.
- the resonant frequency of the quartz crystal drops to a lower level.
- a sample of the detection object is injected to the surface of the QCM/QCM-D chip 20 .
- the resonant frequency increases to a medium level due to the light irradiation on the surface of the QCM/QCM-D chip 20 .
- FIG. 2B is a data graph for detecting the change of concentration of phosphate buffer solutions (PBS) at different concentrations by the novel light-assisted quartz crystal microbalance 2 according to the present invention, wherein the resonant frequency changes with time (unit: minute).
- PBS phosphate buffer solutions
- the irradiation 28 on the surface of the QCM/QCM-D chip 20 causes the increase of the resonant frequency of the chip, and then the resonant frequency decreases after the irradiation is cut off. Then, at time e, 0.016 mmol/L PBS buffer solution is injected to the surface of the QCM/QCM-D chip 20 .
- the grating unit 10 is opened again for irradiation. It can be seen that the irradiation 28 on the surface of the QCM/QCM-D chip 20 causes the increase of the resonant frequency of the quartz crystal. After that, the irradiation is cut off, consequently the resonant frequency decreases again.
- FIG. 2B shows that the light irradiation on the surface of the QCM/QCM-D chip 20 can be utilized to enhance the resonant frequency signal (frequency 28 ) of the quartz crystal, so as to detect the concentration change of PBS buffer solution at low concentration.
- the resonant frequency curve increases by about 2.4 Hz; especially when the detection object ⁇ 0.016 mmol/L PBS buffer solution is switched to pure water, the resonant frequency curve increases by about 1 Hz.
- FIG. 3 is a data graph showing the change of the resonant frequency signal 28 of the QCM/QCM-D chip 20 over time when the same PBS buffer solution shown in FIG. 2B is injected as the detection object, without irradiation on the surface of the QCM/QCM-D chip 20 . It can be seen: when 0.08 mmol/L PBS buffer solution is injected at time d, the resonant frequency increases slightly. Then, as shown at time e, when 0.016 mmol/L PBS buffer solution is injected, the resonant frequency of the quartz crystal further increases slightly; after that, as shown at time f, when pure water is injected for detection, the resonant frequency changes indiscernibly.
- FIG. 3 shows that the resonant frequency change of the quartz crystal resulted from 0.08 mmol/L PBS buffer solution, 0.016 mmol/L PBS buffer solution and 0 mmol/L PBS buffer solution (pure water) is too small to be detected, after the irradiation on the surface of the QCM/QCM-D chip 20 is cut off. Therefore, the change of the resonant frequency of traditional quartz crystal is not enough to distinguish the concentration change of 0.08 mmol/L, 0.016 mmol/L and 0 mmol/L. Hence, the sensitivity of the system is improved with the application of irradiation.
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PCT/CN2017/115776 WO2019109368A1 (en) | 2017-12-07 | 2017-12-13 | Novel light-assisted quartz crystal microbalance and measurement method thereof |
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CN110426451B (en) * | 2019-07-15 | 2021-12-24 | Tcl华星光电技术有限公司 | Etching rate measuring device and lateral etching rate measuring method |
CN114184671B (en) * | 2021-12-09 | 2024-02-06 | 中国石油大学(北京) | Method for determining the number of adsorption layers of a surfactant on a rock surface |
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US20180299410A1 (en) * | 2015-10-14 | 2018-10-18 | Quansor Corporation | Continuous flow fluid contaminant sensing system and method |
US20170260629A1 (en) * | 2016-03-08 | 2017-09-14 | Ultratech, Inc. | Quartz crystal microbalance assembly for ALD systems |
CN106092802A (en) | 2016-05-10 | 2016-11-09 | 浙江大学 | A kind of light swashs the EL-QCM-D array fluid detection system that electricity picks up |
CN107290240A (en) | 2017-07-27 | 2017-10-24 | 江苏集萃有机光电技术研究所有限公司 | QCM and detection method |
CN107917955A (en) | 2017-12-07 | 2018-04-17 | 江苏大学 | New light auxiliary quartz crystal microbalance and its detection method |
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CN107917955A (en) | 2018-04-17 |
WO2019109368A1 (en) | 2019-06-13 |
CN107917955B (en) | 2019-12-03 |
US20210072188A1 (en) | 2021-03-11 |
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